반응 #60662

ord-b538d16793344b958f75b279f78671ff

용매

반응 조건

온도
170°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과was filtered off
  2. 2
    추출the solvent was extracted between H2O and EtOAc
  3. 3
    건조The organic phase was dried over Na2SO4
  4. 4
    기타evaporated
  5. 5
    workup.ADDITIONHeptane:EtOAc 2:1 was added to the residue
  6. 6
    여과the crystalls was filtered off 1.42 g (50%)

실험 절차

2,5-dichloropyridine (1.48 g; 10 mmol), 4-methylsulfonylphenol (1.89 g; 11 mmol) and Cs2CO3 (4.24 g; 13 mmol) was slurried in 75 mL of NMP. The slurry was heated to approx 170° C. over night. After cooling the Cs2CO3 was filtered off and the solvent was extracted between H2O and EtOAc. The organic phase was dried over Na2SO4 and evaporated. Heptane:EtOAc 2:1 was added to the residue and the crystalls was filtered off 1.42 g (50%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07427631B2uspto-grants-2008_09